JP2526281B2 - Method for concentrating polymer solution and filter device thereof - Google Patents

Abstract

PCT No. PCT/DE88/00394 Sec. 371 Date Feb. 15, 1990 Sec. 102(e) Date Feb. 15, 1990 PCT Filed Jun. 28, 1988 PCT Pub. No. WO89/00285 PCT Pub. Date Jan. 12, 1989.The invention relates to a method for concentrating macromolecular solutions, more particularly of protein molecules, to a defined end volume lying in the ul-range and to a filter for carrying out the method. The liquid phase of any amounts of solutions is pressed through an upright filter leaf. The filtered constituents are directed down through gravity and are collected in a concentrate chamber.

Description

FIELD OF THE INVENTION The present invention relates to a method for concentrating a polymer solution and a filter device for carrying out the method.

Background Art W Grace & Company-Amicon Gaem Behr Witten (WRGrace &
Co-AMICON GMBH Witten) Amicon Division No. 1/130 F discloses a general purpose disposable ultrafilter for static concentration of small polymer solutions. The ultrafilter has eight upstanding chambers separated from each other that can be used at different times for different solutions. These chambers are separated by an upright membrane member having an arbitrary permeability. An absorbent material is placed on the back of these membrane members. The absorbent material absorbs the liquid phase portion from the solution in the chamber into the absorbent material by capillary action. The polymeric component is thus concentrated in the solution that remains in the chamber. Therefore, the solution level in the chamber drops. The chamber is marked to indicate the degree of concentration, and as soon as the level of residual liquid reaches the desired mark in the chamber during concentration, the concentrate containing the macromolecules will be concentrated in the chamber. Taken from. The lower portion of the membrane member is made impermeable to prevent further concentration. Such a well-known concentration method is performed in a batch system. Therefore, when the liquid phase component is removed, the necessary solute component is concentrated in the residual liquid. Such a concentration process is limited by the capacity of the absorbent material. When trying to concentrate a large amount of solution, this method makes the operation method very complicated. It cannot be said that the desired constant concentration can be obtained at any level. In this method, when the liquid phase component is absorbed through the membrane member, a part of the polymer is deposited on the membrane member.
Such a polymer remains attached to the membrane member and does not enter the concentrate even if the level surface of the solution is further lowered.
This material loss greatly reduces the efficiency of the above concentration method.

Column 1, 37 of US Patent No. 4632761
In lines 41 to 41, the concentrated component filtered by the surface tension acting on the concentrate in the region of the filter part that became impermeable due to the capillary phenomenon only in the ultrafilter described above was completely dry. Is emphasized and explained. The product can thus be rendered useless, and the risk of producing such a dry condition has been pointed out by the manufacturer in a notice included with the ultrafilter.

U.S. Pat. No. 4,123,224 also discloses a method and device for concentrating a solution containing a polymer. The solution is introduced into the concentration chamber defined by the filter. An absorbent material is provided on the filtrate side of the filter. The concentrate is collected in a concentrate (container) chamber adjacent to the concentrate chamber. The filter surface is reduced towards the concentrate chamber. The concentrate is collected in the concentrate chamber in a limited final volume separated from the filter leaf.

OBJECT OF THE INVENTION It is an object of the present invention to provide a concentration method capable of performing an ideal yield or concentration of a solution in a predetermined range including a considerably small volume, and a filter device therefor.

DISCLOSURE OF THE INVENTION Advantageously, a controllable pressure is applied to the solution to be concentrated, whereby it is pressed along the filter leaf into the concentration chamber. Adjustable pressure and choice of filter material can achieve ideal results in the filtration process. Further, during the concentration of the solution, a flow is generated from the concentration chamber into which the solution has been injected, toward the concentrate (accommodation) chambers arranged in series therebelow, and the polymer component concentrated by the fluid component is generated. Easily integrated in the concentrate chamber. Since it is not necessary to temporarily lower and observe the solution level in the concentration chamber during the concentration operation, there is no risk of the concentration chamber becoming particularly dry. Further, such concentration operation can be performed at a higher concentration in connection with the analysis work for obtaining greater accuracy.

One of the advantageous ways to promote concentration is to concentrate the concentration of the filter at the site where the filter surface near the boundary point between the concentration chamber and the concentrate chamber is narrowed if the solvent is expelled through the filter. More improved.

On the contrary, the concentration method according to the invention has the advantage that the solution can be pre-concentrated in at least one large volume pre-filter step. Such preconcentration can be carried out, for example, in a cascade type prefilter. In order to retain the moisture content of the concentrate, it is desirable to prevent the filter leaf from acting directly on the concentrate (container) chamber, with a hydrophobic mask covering the part of the filter leaf to be deactivated. It is advantageous to cover.

According to the present invention, the solution carries its solvent through the filter leaf to the drainage channels juxtaposed to the outside, and the remaining concentrated polymer component is pumped along the filter leaf.
The polymer component is less likely to adhere to the inner surface of the filter leaf, and can be sequentially pushed by the inflowing solution and efficiently collected in the lower concentrate chamber. In addition, backflushing the filter leaf at an appropriate time is also advantageous because it removes deposits on the leaf surface.

In the present invention, it is possible to apply an adjustable pressure to the solution by means of a load or air pressure, a hydraulic pressure or a motor driven pump.

In order to further reduce the liquid content of the filtered macromolecular concentrate, it is advantageous to apply a centrifugal force to at least the concentrate when it is desirable or essential.
A centrifuge or pendulum can be used for this. Such centrifugal force can advantageously generate an adjustable pressure on the object, resulting in a proper amount of liquid phase separation.

Next, a filter device for carrying out the above concentration method will be described. The device is advantageously constructed as a sandwich structure with two discs sandwiching the filter part.
One of the discs is a filter chamber disc which forms a concentrating chamber therein, the concentrating chamber having a generally elongated hexagonal profile with two parallel sides and two pairs of converging equilateral sides. And the lower side pair is connected to a channel chamber containing the concentrate. In addition, the filter chamber disc has a mask which is mounted in a recess containing the concentration chamber, the mask having an aperture which matches the contour of the concentration chamber and a part of the concentrate chamber. . The mask is overlaid with an ultrafilter leaf of sufficient size to cover the opening in the mask. The filter chamber disc is further combined with a filter support disc including channels for discharging the solvent liquid passing through the filter to form a sandwich structure.

The upper end of the concentration chamber is connected to the supply channel of the solution to be concentrated, which solution is pressed along the front face of the filter. The concentrated components resulting from the filtration can flow further downward toward the concentrate chamber by the lower equilateral side pairs. At the time of injecting the solution to be concentrated, the air and gas in the concentration chamber are easily discharged upward.

By forming a peripheral bead on the edge of the hexagonal concentrating chamber and the concentrating chamber connected thereto, a reliable sealing of the concentrating chamber and the concentrating chamber can be performed with respect to the sheet-shaped mask and filter leaf.

For ideal concentration, it is preferred that the depth of the concentration chamber be shallow from the portion following the liquid supply channel to the concentrate chamber below.

It should be noted that the liquid supply channel may be equipped with a Luer-Lock lid so that the tip of a dropper used to take out the concentrated polymer component can be easily passed therethrough. In order to ideally seal the edge of the concentration chamber and the filter member, a contact pressure receiving portion is formed on the filter supporting disk. The contact pressure receiver covers the peripheral bead of the concentration chamber and has at least three parallel open channels for the filter leaf in the surface water region inside the peripheral bead of the concentration chamber. The lower ends of these parallel open channels are connected to a single open channel formed in the surface area inside the peripheral beads of the concentrate chamber,
This open channel leads to an outlet formed in the lower part of the filter support disk. Sandwich structure 2
When the two discs are tightened, the contact bearings press the rectangular mask and filter leaf fitted between the two discs against the peripheral bead of the filter chamber disc, providing a secure seal. In order to fix the filter leaf and the mask placed inside the sandwich structure in place, these membrane members and the discs on both sides have aligned holes and at least two fixing pins are inserted through them. .

In a preferred embodiment, the filter chamber disc described above has a parallelepiped open recess,
A concentrate chamber and a concentrate chamber are formed at the bottom of the recess. The filter support disc facing it has a parallelepiped web of the same shape, which is hermetically mounted in the recess and has a contact pressure receiving part on the face of the two chambers. Such an embodiment allows the components to be quickly assembled into a sandwich structure. In order to facilitate the insertion of the mask and ultra filter at the time of assembly and removal of the filter leaf and the mask after filtration, a pair of overhanging curved surfaces is provided at the upper end of the side wall of the parallelepiped-shaped recess, such as a filter leaf. The air inside the filter leaf is allowed to flow out through these curved surfaces during insertion. Two recessed grooves are formed on the open edge of the bottom of the parallelepiped recess. The filter leaf and the mask can be easily removed from the recess by inserting an auxiliary tool into these grooves. In order to hold the sandwich structure thus composited in that state,
At least two pairs of holes are provided in the filter chamber disc and the filter support disc. These hole pairs are aligned with each other and are adapted to be inserted through a sandwich-type tightening member. Further, when the filter device of such an aspect is attached to a centrifuge or other device in order to provide an additional filtering capacity, the filter chamber disc and the filter support disc are formed into complementary cylindrical shapes, and the filtration is performed. It is desirable to keep the surface in an outward arc shape.

 Embodiments of the present invention will be described below with reference to the drawings.

BRIEF DESCRIPTION OF THE DRAWINGS FIGS. 1 and 2 are a plan view and a sectional view of a filter chamber disc according to an embodiment, and FIGS. 3 and 4 are a side view and a plan view of a filter support disc assembled to the filter chamber disc. FIG. 5 and FIG. 5 are plan views of the mask, and FIG. 6 is a side view showing the sandwiched filter device in a tightened state.

Embodiment The filter chamber disc 1 shown in FIG. 1 has a parallelepiped-shaped recess 45 whose lower part is open. The hexagonal outer shape of the concentrating chamber 2 is formed in a bottom portion 46 of the recess 45 at a substantially central portion thereof. Concentration chamber 2 has two parallel sides 2
Divided by 6,27. These parallel sides 26,27
The upper end of is connected to the equilateral side pair 28. The upper corner of the chamber 2 formed by these equilateral side pairs 28 leads to a liquid supply channel 41 with a Luer-Lock lid 43. The lower ends of the parallel sides 26, 27 of the concentration chamber 2 are connected to the equilateral side pair 29. Advantageously, the length of the sides of these side pairs 29 is longer than the length of the upper, opposite side pair 28. Concentration chamber 2
The lower corner is formed by a downwardly converging side pair 29, which is a concentrate chamber with a closed bottom end.
31 that is, it is connected to the groove where the concentrate is collected.
Bottom of the recess 45 on both sides of the lower side pair 29 of the concentration chamber 2.
The rectangular general ultrafilter leaf (not shown) (not shown) and a pin 48 for fixing the mask 33 (FIG. 5) are provided at 46.

As shown in FIG. 3, the filter support disk 35 has a parallelepiped-shaped web 53 on one side surface, and this web 53 can be mounted in the recess 45 of the filter chamber disk 1 in a sealed state. . On the side surface 54 of the web 53, a contact pressure receiving portion 44 is provided so as to project, and the contact pressure receiving portion 44 covers the peripheral beads 42 of the concentration chamber 2 and the concentrate chamber 31 in the filter chamber disk 1 in the assembled state. It is like this. The contact pressure receiving portion 44 is a peripheral bead.
It is designed with a slightly larger external size to fit the 42 shape. The contact pressure receiving portion 44 is formed with three parallel open channels 36, 37 and 38, the lower ends of which are connected to one open channel 39. In the assembled state, the channels 39 are located opposite the concentrate chamber 31 and are separated from each other by part of the ultrafilter leaf or part of the mask. The channels 36, 37, 38, 39 are open at the front. The channel 39 is connected to an outlet 40 that laterally exits the body of the filter support disk 35.
The discharge port 40 delivers the solvent that has passed through the filter or the like.

Filter chamber disc 1 and filter support disc
35 has a plurality of common bolt holes 50 and 51, and tightening bolts are inserted into the holes 50 and 51 when the sandwich structure of both discs 1 and 35 is assembled, and the filter chamber disc 1 and the filter support disc 35 are Are crimped together (see FIG. 6).

When assembled in the sandwich structure as above,
A mask 33 of the hydrophobic material shown in FIG. 5 is first placed on the peripheral beads 42 in order to eliminate capillary action. The mask 33 has an opening 34 which is shaped to match the side edges of the concentrating chamber 2 and thus the peripheral beads 42. The opening 34 also has a groove 55 at its lower end that covers only the upper portion 32 of the concentrate chamber 31. Therefore this groove
The length of 55 is shorter than the total length of the concentrate chamber 31, and the mask 33
The shielded area by means of which determines the final set volume of concentrate.

The same rectangular ultra filter leaf is placed on the mask 33 and is aligned by the fixing pin 48.

The web 53 of the filter support disc 35 is a fixing pin.
By inserting the hole 48 into the hole 49, the hole 48 can be easily mounted in the recess 45 of the filter chamber disc 1.

The sandwich structure described above can thus be crimped together through the pins 60 in the holes 50,51.

The solution is introduced under pressure into the concentrating chamber 2 through the part of the Luer-Rock lid 43, and then the filter leaf is crimped between the peripheral bead 42 of the filter chamber disc 1 and the contact pressure receiving part 44 of the filter support disc 35. Through (not shown), the solvent is pressed into the open channels 36, 37, 38 on the side of the filter support disk 35. Concentration chamber 2
The polymer separated by separating the solvent inside is concentrated in the chamber 2.
It settles down and slides down along the converging side pair 29. The upper portion 32 of the concentrate chamber 31 is still filtering. As a result, a downwardly flowing fluid component is generated with respect to the polymer concentrate that settles downward, and the polymer is accumulated in the concentrate chamber 31 especially in the lower half thereof by the action of such fluid components in addition to gravity. It If the polymer adheres considerably to the inner surface of the filter leaf during concentration, the lock lid is temporarily closed, and the solvent is adjusted so that a pressure gradient in the opposite direction occurs on the filter leaf surface from the outlet side connected to the discharge port 40. By pressurizing, the polymer can be separated from the filter leaf to the inside, returned to the solution in the concentration chamber 2 and allowed to settle in the concentrate chamber 31.

As shown in FIG. 1, two outwardly curved surfaces 61 are provided on the upper side of the recess 45 of the disc 1 so that air is released when the rectangular filter leaf is mounted. be able to. Further, at the bottom of the recess 45, two recesses 57 are provided on the bottom surface. When the filtration process is completed, the mask and the filter leaf can be lifted and removed by an auxiliary tool inserted into these grooves 57. As shown in FIG. 6, tension pins or bolts 60 are inserted into the holes 50 and 51 described above. This tension pin 60
Supports a tension web 58 to which a tightening screw 59 is screwed, so that the sandwich members can be pressed together.

After the concentration process, the concentrate, such as the polymer, is removed from the concentrate chamber 31, for example by a dropper inserted through the channel 41 during filling.

Claims (23)

(57) [Claims] 1. A method for concentrating a solution containing macromolecules, in particular a solution containing protein molecules, to a predetermined final volume, the one side being defined by a flat filter leaf,
A solution is press-fitted along the filter leaf from above into a concentration chamber having a filtration surface that narrows toward the lower concentrate chamber, and while separating the solvent through the filter leaf, the resulting concentrate flows in the concentration chamber. The concentrate is collected in the concentrate chamber that continues downward, and further, in the concentrate chamber, an upper filtration region facing the filter leaf and a lower masking region by a mask covering the leaf are formed in advance to concentrate the concentrate. Wherein the flowable component containing is subsequently filtered in the upper filtration region of the concentrate chamber to finally concentrate the filtered polymeric component to a predetermined volume in the lower shielding region in the concentrate chamber. A method for concentrating a polymer solution. 2. A solution is passed through the filter leaf at an adjustable pressure in the concentrating chamber, and the filtrate flows in the concentrating chamber mainly along a filtering surface into the groove-shaped concentrating chamber. The concentration method according to claim 1, wherein the concentration method is performed. 3. The concentration method according to claim 2, wherein the solvent separated through the filter leaf is collected through a channel-shaped discharge passage on the filter leaf supporting side. 4. The solution is pre-concentrated in an appropriate number of stages by a cascade type pre-filter.
The concentration method according to at least one of 3 to 3. 5. The concentrate chamber and a part of the concentrate chamber are shielded on one side by the filter leaf, and the rest of the concentrate chamber is shielded by a mask made of a hydrophobic material. Claim 1 to
4. The concentration method according to at least one of 4. 6. The concentration method according to claim 1, wherein the filter leaf is backflushed in a timely manner. 7. When the polymer adheres to the inner surface of the filter leaf, the solvent side is pressurized so that the pressure gradient of the filtrate on the filter leaf surface occurs in the direction opposite to the filtration pressure gradient. 7. The concentration method according to at least one of to 6. 8. A method according to claim 1, wherein the adjustable pressure is generated in the solution by load, air pressure, hydraulic pressure or a motor driven pump. 9. A centrifugal force is applied to at least the concentrate to further reduce the liquid content.
~ 8. The method according to at least one of 8. 10. At least one of claims 1 to 9, characterized in that the concentrate, such as a polymer, is withdrawn from the concentrate chamber by means of a suction device inserted through the filling channel.
Concentration method described in 3. 11. A filter device for concentrating a solution containing a polymer to a predetermined final volume, which comprises side portions (26, 27) parallel to each other and two pairs of equilateral converging side portions (upper and lower sides). 2
A concentrating chamber (2) with a hexagonal outer shape having a converging end formed by a lower side pair (29) leading to a groove-shaped concentrating chamber (31) on one side. A filter chamber disc (1) having a surface, a hexagonal outer shape (26,27,28,29) of the concentration chamber (2) and a concentrate chamber (2) placed on one side of the filter chamber disc (1) The opening (3) that matches the upper part (32) of the (31)
4,35) and a mask (33) made of a hydrophobic material, an ultrafilter leaf placed on top of the mask (33), open channels (36-39) for receiving the liquid phase of the solution, and an outlet. (40) and a filter device having a sandwich structure including a filter support disk (35) mounted and tightened on the filter chamber disk (1). 12. A peripheral bead (42) is provided at the edge of the hexagonal concentrating chamber (2) and the channel-shaped concentrating chamber (31) connected therebelow. The filter device according to item 11. 13. The filter device according to claim 11, wherein a solution supply channel (41) is connected to a corner of an upper end of the concentration chamber (2). 14. Filter device according to claim 13, characterized in that the solution supply channel (41) comprises a Luer lock lid (43). 15. Filter device according to claim 13 or 14, characterized in that the depth of the concentration chamber (2) is shallower from the solution supply channel (41) towards the concentrate chamber (31). 16. The filter support disk (35) is provided with a contact pressure receiving portion (44) which covers the concentration chamber (2) and a peripheral bead (42) of the concentrate chamber (31).
The contact pressure receiving part (44) has at least three parallel open channels (36, 37, 38) in the surface area inside the peripheral bead (42) of the concentration chamber (2), and these open channels are concentrated. At least one of claims 11 to 15, characterized in that it leads to an open channel (39) formed in the surface area inside the peripheral bead (42) of the article chamber (31) and further to an outlet (40). The filter device according to one. 17. The filter chamber disc (1) has at least two fastening pins (48) and the filter support disc (35) has at least two holes (49) for receiving said pins (48). A filter device according to at least one of claims 11 to 16, characterized in that it comprises. 18. The filter chamber disc (1) has an open recess (45) of parallelepiped, the bottom (46) of which has the concentration chamber (2) and the concentration chamber (31) formed therein. The filter support disk (35) has a parallelepiped-shaped web (53) fitted in the recess (45) in a sealed state, and the contact pressure receiving portion (44) has a web (53).
It is formed on the end surface of
The filter device according to at least one of items 1. 19. A parallelepiped recess (45) has an upper end formed with a curved surface (61) for venting air on both sides, and an opening end of the recess (45) for removing a filter leaf. 19. Filter device according to claim 18, characterized in that two grooves (57) are formed. 20. The filter chamber disc (1) and the filter support disc (35) are provided with at least two mutually opposing pairs of holes (50,51), which holes (50,51) are provided. 20. The filter device according to at least one of claims 11 to 19, characterized in that a tightening member (60) for the sandwich structure is inserted. 21. The filter device according to claim 11, wherein the filter chamber disc (1) and the filter support disc (35) are designed as complementary partial cylinders. . 22. The concentrate chamber (31) is partially shielded from the filter leaf by a mask (33) made of foil or Teflon.
Filter device according to at least one of 21. 23. Filter device according to claim 22, characterized in that the mask (33) made of foil or Teflon has a thickness of 0.25 mm to 0.75 mm, in particular 0.5 mm.